反应详情

The phosphinate ester product of Example 16 (220 g) was refluxed 2 hr with aqueous sodium hydroxide (2 N: 660 ml). The cooled solution was taken to pH 7.0 with conc. hydrochloric acid, evaporated in vacuo and the solid residue was triturated with methanol and insoluble material filtered off. The filtrate was again evaporated to dryness, the residue triturated with methanol and further insoluble material filtered off. The filtrate was finally evaporated to dryness, triturated with acetone and filtered to give the title compound (2.9 g) mp 258°-262° C., identical (ir nmr) with the product from Example 17.

1. customevaporated in vacuo
2. customthe solid residue was triturated with methanol and insoluble material
3. filtrationfiltered off
4. customThe filtrate was again evaporated to dryness
5. customthe residue triturated with methanol and further insoluble material
6. filtrationfiltered off
7. customThe filtrate was finally evaporated to dryness
8. customtriturated with acetone
9. filtrationfiltered